U.S. patent number 7,550,197 [Application Number 11/776,025] was granted by the patent office on 2009-06-23 for non-toxic flakes for authentication of pharmaceutical articles.
This patent grant is currently assigned to JDS Uniphase Corporation. Invention is credited to Alberto Argoitia, Paul G. Coombs, Wilfred C. Kittler, Jr., Charles T. Markantes.
United States Patent |
7,550,197 |
Kittler, Jr. , et
al. |
June 23, 2009 |
Non-toxic flakes for authentication of pharmaceutical articles
Abstract
In one embodiment of the present invention, non-toxic inorganic
flakes are used for identification and anticounterfeit protection
of pharmaceutical articles, such as pills, tablets and capsules,
having a core of a biologically active material and/or a
biologically inert material. Non-toxic inorganic authentication
flakes, either optically variable flakes or taggant flakes having
one or more symbols and/or a selected shape are disposed on the
surface or inside of the pharmaceutical article.
Inventors: |
Kittler, Jr.; Wilfred C.
(Rohnert Park, CA), Argoitia; Alberto (Santa Rosa, CA),
Coombs; Paul G. (Santa Rosa, CA), Markantes; Charles T.
(Santa Rosa, CA) |
Assignee: |
JDS Uniphase Corporation
(Milpitas, CA)
|
Family
ID: |
38971656 |
Appl.
No.: |
11/776,025 |
Filed: |
July 11, 2007 |
Prior Publication Data
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Document
Identifier |
Publication Date |
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US 20080019924 A1 |
Jan 24, 2008 |
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Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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10641695 |
Aug 14, 2003 |
7258915 |
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60807097 |
Jul 12, 2006 |
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Current U.S.
Class: |
428/323; 428/328;
428/403; 428/407 |
Current CPC
Class: |
A61K
9/2813 (20130101); A23L 29/015 (20160801); A23L
33/16 (20160801); Y10T 428/25 (20150115); Y10T
428/2998 (20150115); Y10T 428/256 (20150115); Y10T
428/2991 (20150115) |
Current International
Class: |
B32B
5/16 (20060101) |
Field of
Search: |
;428/323,328,403,407 |
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|
Primary Examiner: Kiliman; Leszek
Attorney, Agent or Firm: Allen, Dyer, Doppelt, Milbrath
& Gilchrist, P.A.
Parent Case Text
CROSS-REFERENCE TO RELATED APPLICATIONS
The present application is a continuation-in-part of U.S. patent
application Ser. No. 10/641,695 filed Aug. 14, 2003 now U.S. Pat.
No. 7,258,915, entitled "Flake For Covert Security Applications",
and claims priority from U.S. Provisional Patent Application Ser.
No. 60/807,097 filed Jul. 12, 2006, entitled "Food Safe Encoded
Microflakes For Pharmaceutical Or Nutriceutical Tablet Labeling"
the disclosures of which is incorporated herein.
Claims
What we claim is:
1. A pharmaceutical, nutraceutical, or veterinarian unit-dosage
article having a surface, comprising: a material selected from the
group consisting of a biologically active material and a
biologically inert material, and a mixture thereof; and
authentication flakes selected from the group consisting of
non-toxic, inorganic optically variable flakes having at least one
metallic layer and non-toxic, inorganic taggant flakes; wherein the
authentication flakes are dispersed within the article or on the
surface.
2. An article defined in claim 1, wherein the material forms a core
of the article; wherein the article further comprises a coating on
at least a portion of the core, and wherein the authentication
flakes are dispersed within the coating.
3. An article defined in claim 2, wherein the core is selected from
the group consisting of a liquid, a powder, and granules, and
wherein the coating forms a capsule case around the core.
4. An article defined in claim 2, wherein the authentication flakes
form less than 10% by weight of the coating.
5. An article defined in claim 1, wherein the authentication flakes
are non-toxic, inorganic taggant flakes having a predetermined
shape.
6. An article defined in claim 1, wherein the authentication flakes
are non-toxic, inorganic taggant flakes having indicia or a grating
pattern thereon.
7. An article defined in claim 1, wherein the authentication flakes
are non-toxic, inorganic taggant flakes having one or more frame
borders along an edge thereof.
8. An article defined in claim 1, wherein the authentication flakes
are non-toxic, single-layer dielectric taggant flakes.
9. An article defined in claim 1, wherein the authentication flakes
are clear or colored taggant flakes.
10. An article defined in claim 1, wherein the authentication
flakes are non-toxic, dielectric covert taggant flakes.
11. An article defined in claim 1, wherein the authentication
flakes are non-toxic taggant flakes comprising a material selected
from the group consisting of zinc, magnesium, iron, titanium, gold,
and silver.
12. An article defined in claim 1, wherein the authentication
flakes are optically variable non-toxic flakes, each comprising a
non-toxic reflector layer, a non-toxic absorber layer, and a
non-toxic dielectric layer therebetween.
13. An article defined in claim 12, wherein the non-toxic absorber
layer comprises a material selected from the group consisting of
iron, zinc, magnesium, iron, titanium, gold, and silver.
14. An article defined in claim 12, wherein the non-toxic reflector
layer comprises a material selected from the group consisting of
zinc, magnesium, iron, titanium, gold, and silver.
15. An article defined in claim 1, wherein the authentication
flakes include a material selected from the group consisting of:
TiO.sub.2, TiO, SiO, SiO.sub.2, ZnO, MgO, and oxides of iron.
16. An article defined in claim 1, wherein the authentication
flakes are dispersed within the article and wherein the
authentication flakes form less than 5% by weight of the
article.
17. An article defined in claim 16, wherein the authentication
flakes are dispersed within the article and wherein the
authentication flakes form less than 1% by weight of the
article.
18. A pharmaceutical, nutraceutical, or veterinarian ointment
comprising: an ointment base selected from the group consisting of
a biologically active material and a biologically inert material,
and a mixture thereof; and authentication flakes selected from the
group consisting of non-toxic, inorganic optically variable flakes
and non-toxic, inorganic taggant flakes; and wherein the
authentication flakes are dispersed within the ointment base.
19. An article defined in claim 18, wherein the authentication
flakes form less than 5% of the ointment by weight.
20. An article defined in claim 18, wherein the authentication
flakes are one selected from the group of taggant flakes having a
predetermined shape, taggant flakes having one or more frame
borders along an edge thereof, taggant flakes having indicia or a
grating pattern thereon, single-layered clear dielectric taggant
flakes, and single-layered colored taggant flakes.
Description
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
REFERENCE TO MICROFICHE APPENDIX
Not applicable.
FIELD OF THE INVENTION
The present invention relates generally to non-toxic inorganic
flakes, and more particularly to their use for authentication of
pharmaceutical, nutraceutical, or veterinarian articles.
BACKGROUND OF THE INVENTION
Specialty pigments have been developed for use in security
applications, such as anti-counterfeiting devices printed on
banknotes, packaging of high-value items, seals for containers, and
even for direct application to commercial items. For example, the
U.S. twenty-dollar Federal Reserve Note currently uses optically
variable ink. The number "20" printed in the lower-right corner of
the face of the note changes color as the viewing angle changes.
This is an overt anti-counterfeiting device. The color-shifting
effect is not reproducible by ordinary color photocopiers, and
someone receiving a note can observe whether it has the
color-shifting security feature to determine the note's
authenticity.
Other high-value documents and objects use similar measures. For
example, iridescent pigments or diffractive pigments are used in
paints and inks that are applied directly to an article, such as a
stock certificate, passport, original product packaging, or to
seals that are applied to an article. Unfortunately, counterfeiters
continue to become more sophisticated. Security features that are
more difficult to counterfeit are desirable.
One anti-counterfeiting approach uses microscopic symbols on
multi-layer color-shifting pigment flakes. The symbols are formed
on at least one of the layers of the multi-layer color-shifting
pigment flakes by a local change of an optical property(s), such as
reflectivity. The multi-layer color-shifting pigment flakes
generally include a Fabry Perot-type structure having an absorbing
layer separated from a reflective layer by a spacer layer. The
reflective layer is typically a layer of metal, which renders the
pigment flake essentially opaque. If a large portion of these types
of pigment flakes are mixed with other pigment, the resultant color
might be significantly different from the pigment.
Clear pigment flakes with holographic information are also used for
anti-counterfeiting purposes. A monochromatic volume hologram is
formed in a polymeric platelet using a reference laser light in the
visible, infrared ("IR"), or ultraviolet ("UV") region. The
polymeric platelet does not have a metallic reflective layer, and
may be mixed in with other coatings, including metallic coatings
(e.g. inks and paints), without disturbing the subjective color
appearance of the coating. The polymeric platelets can also be
incorporated in a varnish coating, which may be applied over an
article without changing its color. When the polymeric platelets
are irradiated with the reference laser light, the hologram may be
read for the information it contains. However, polymeric materials
may break down in sunlight and holograms have become relatively
easy to counterfeit because an original hologram can provide a
"fingerprint" (template) that facilitates copying. Holograms are
not as strong an anti-counterfeiting device as they used to be.
It is desirable to mark objects with covert anti-counterfeiting
devices that overcome the limitations of the techniques discussed
above.
BRIEF SUMMARY OF THE INVENTION
A coating composition includes covert flakes with identifying
indicia made of a single layer of inorganic dielectric material.
Examples of identifying indicia include selected flake shape(s)
and/or symbol(s). The covert flakes are typically dispersed in a
carrier, such as a varnish base, paint vehicle or ink vehicle, to
form a coating composition. The covert flakes are dispersed in
sufficiently dilute concentration so that the covert flakes are not
easily detectable in the coating composition by casual observation
and can be clear or colored to match the color of a base
pigment.
In a particular embodiment, covert security flakes fluoresce when
illuminated with non-visible radiation. In an embodiment of the
invention, fluorescing covert security flakes make up less than 1%
of the composition.
In another embodiment, clear covert flakes in a varnish composition
make up to 20% of the composition. In another embodiment, clear
covert flakes make up to 10 weight percent of a total pigment
weight in a composition having optically variable base pigment
flakes.
In a particular embodiment the covert flakes are a single layer of
an inorganic dielectric material, such as ZnS. The thickness of the
single layer of inorganic dielectric material is selected to
provide a covert flake that has color, or that is clear. In a
further embodiment, clear covert flake is heat-treated to improve
its clarity (i.e. "whiteness").
In another embodiment, a coating composition has clear covert
flakes that are not easily detectable in the coating composition by
observation under visible light dispersed in a carrier. The clear
covert pigment flakes fluoresce when illuminated with UV light and
have one or more symbols readable under visible light at a
magnification of 50.times.-200.times. In a particular embodiment,
the clear covert flakes in the carrier have a transmittance of more
than 70% in the visible region.
A composition according to an embodiment of the present invention
is applied to an object to provide a covert security feature. A
pigmented composition may be used to print a field (e.g. an image)
on the object, and a varnish composition may be used to print a
clear field on the object, or to overprint an existing image on the
object. In an embodiment of the invention, covert flake is mixed
with base pigment to provide a covert security feature to images
printed with the composition that look substantially similar to
images printed with the base pigment.
In a method according to an embodiment of the present invention,
symbols on covert flakes are not readable when the covert security
feature is illuminated with non-visible radiation, i.e. when the
flake is fluorescing. The location of a covert flake is identified
using non-visible radiation, and then the flake is observed under
visible light (typically under magnification of
50.times.-200.times.) to read the symbol(s) on the covert
flake.
In one embodiment of the present invention, non-toxic inorganic
flakes are used for identification and anticounterfeit protection
of pharmaceutical, nutraceutical, or veterinarian unit-dosage
articles, such as pills, tablets and capsules, having a core
essentially consisting of a biologically active material and/or a
biologically inert material. Non-toxic inorganic authentication
flakes, either optically variable flakes having at least one
metallic layer or taggant flakes, are disposed within the core or
on the surface of the article.
In another embodiment of the present invention, non-toxic inorganic
authentication flakes are dispersed within a pharmaceutical,
nutraceutical, or veterinarian ointment.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a plan view of a portion of a document with a security
feature according to an embodiment of the present invention.
FIG. 2A is a simplified plan view of a portion of a security
feature according to an embodiment of the present invention.
FIG. 2B is a simplified plan view of a portion of a security
feature according to another embodiment of the present
invention.
FIG. 2C is a simplified plan view of a portion of a security
feature according to yet another embodiment of the present
invention.
FIG. 3 is a cross section of a varnish with clear covert flakes
dispersed in a carrier according to an embodiment of the present
invention.
FIG. 4 is a cross section of base flakes and covert flakes
dispersed in a binder according to another embodiment of the
present invention.
FIG. 5A is a simplified plan view of a portion of a security
feature printed with clear, inorganic covert flake according to an
embodiment of the present invention as seen under a microscope
using UV illumination.
FIG. 5B is a simplified plan view of the portion of the security
feature of FIG. 5A as seen under a microscope using visible light
for illumination.
FIG. 6 shows the color travel for a test sample prepared with an
ink, and for test samples prepared with the ink in combination with
covert pigment flakes according to an embodiment of the present
invention.
FIG. 7 is a simplified flow chart of a method of observing covert
flakes according to an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
I. Introduction.
Flakes for covert security applications are not typically seen by
casual observation. Some sort of inspection technique, such as
inspection under a microscope or illumination with a particular
type of light, is used to find and/or read the flakes. Flakes
according to embodiments of the invention can be colored ("pigment
flakes") or essentially clear.
In one embodiment, flakes containing indicia, such as a symbol or a
particular shape, substantially match the visual characteristics of
a bulk pigment or other substance they are mixed with. In a
particular embodiment, a single-layer inorganic flake having a
selected shape or symbol is mixed with an iridescent mica-based
flake or other base pigment. In another embodiment, clear flakes
having indicia are mixed with bulk pigment without disturbing the
visual characteristic of the resultant mixture. In yet another
embodiment, clear flakes having indicia are mixed in a varnish and
applied over an object to provide a covert security feature without
substantially changing the underlying color. As used herein, a
varnish is generally a substantially clear composition.
In a particular embodiment, flakes made from a single-layer of ZnS
are heat-treated to whiten or "bleach" the appearance of the flake
and improving the clarity (i.e. reducing the yellow nature) of the
resultant composition. For the purpose of this discussion, a
"single layer" of inorganic material includes multiple layers of
the same inorganic material built up upon each other.
In yet another embodiment, covert flakes are mixed with a chemical,
such as an explosive, explosive precursor, food, drug, or
controlled substance. The covert flakes include indicia, such as
symbols and/or other patterning (e.g. grooves) and specific shapes
that identify the manufacturer or provide other specific
information. Inorganic flakes are particularly desirable in
applications where heat, solvents, sunlight, or other factors may
degrade organic flakes. For example, an inorganic covert flake used
in an explosive is detectable even after exposure to high
temperatures and/or pressures, and is persistent in the
environment.
In a particular embodiment, authentication flakes including OV
flakes and taggant flakes are used for labeling pills, tablets,
suppositories, capsules, or ointments containing biologically
active material. Alternatively, the biologically active material
can be added or replaced by a biologically non-active material, for
example for placebo trials.
Many materials conventionally used for optical flakes are not safe
for ingestion. In particular, Zinc sulfide is an irritant when
ingested due to the production of hydrogen sulfide. Some materials,
like lead, arsenic, and cadmium, are poisonous or carcinogenic.
Other materials can only be used in very trace amounts, for
example, selenium, chromium or cobalt; heavy metals must be limited
in their dosage. Aluminum is often referred as harmful material,
however it is a component of certain antacids, and some baking
powders contain sodium aluminum sulfate. Safety of a particular
material depends on an amount ingested and should be evaluated
separately for different patient groups.
For use in the pharmacology or food industry, the authentication
flakes are made of non-toxic, preferably inert, materials. The term
"non-toxic" is used here in its broadest sense meaning that the
substance is not harmful and may be safely ingested. The non-toxic,
or edible, authentication flakes are applied on the surface or
within pills, tablets, suppositories, or capsules containing
liquid, powdered, or granulated medicine. Alternatively, the
authentication flakes are used in a pharmaceutical, nutraceutical,
or veterinarian ointment as dispersed within an ointment base.
In accordance with the present invention, inorganic compounds like
silica, titania, alumina, are used in non-toxic authentication
flakes, since they are inert and safe to ingest, and they are
persistent and detectable by their difference from the organic
materials of the coating or tablet under a microscope.
Non-toxic dielectric materials include inert materials, such as
SiO.sub.2, and materials approved by the FDA as food additives and
colorants, such as iron oxides and titanium oxides. Other
materials, such as MgO and ZnO are actually nutrients and are
acceptable in small quantities. MgO is used as an antacid, and has
a Recommended Daily Allowance (RDA) of about 300 milligrams or
more. ZnO is also a micronutrient and has an RDA of 10-15
milligrams.
Some of the dielectric materials are clear materials, including
SiO2 and TiO2, MgO and ZnO. Other non-toxic dielectric materials,
such as SiO, Iron oxides and some of the Ti oxides are absorbing
depending on their degree of oxidation. Doped dielectric materials,
such as Fe doped SiO2, Ti doped Al203, etc, are colored dielectric
materials. In some embodiments, the flakes are thermally treated to
achieve a desired coloration. Also, irradiation of dielectric
materials is used in Jewelry industry to induce color. Such
materials are used in single layered colored taggant flakes.
Non-toxic dielectric materials are used, in particular, for
manufacturing single-layered taggant flakes, clear or colored, as
described hereinbelow. Preferably, taggant flakes are single
layered to reduce the amount of "foreign" material delivered to the
organism; however, authentication flakes can consist of more than
one layer. Flakes having an absorbing dielectric layer over a
reflector layer exhibit a strong coloration, which is dependent on
both thin film interference effects and the intrinsic coloration or
absorbance of the material itself. Even a weakly absorbing
dielectric layer together with a reflector layer provides a vivid
effect vivid, with the quite bright reflectance.
Non-toxic authentication flakes require materials which are
physiologically inert, like aluminum oxide, titanium dioxide, the
silicon oxides, and iron oxides. Preferred metals for use in
authentication flakes are well tolerated by the body and considered
a part of a normal diet.
Metals such as titanium, gold, silver, zinc, magnesium, iron, or
metal compounds such as carbides or nitrides, for example, TiN,
TiC, TiOxCyNz, etc, are used in non-toxic flakes to improve
visibility and add coloration, and add overt recognition without
compromising edibility. Despite small particles of iron are easily
absorbed, the total amount of iron in flakes on one pill is about a
few micrograms, whereas over-the-counter vitamins typically contain
18 milligram of iron per pill. Chromium is also used as a food
supplement in amounts above 100 microgram a day. Many metals are
tolerated and even required by the body in small quantities. There
are medical references to the body's need for trace metals, see for
example
http://www.merck.com/mmhe/sec12/ch155/ch155a.html#tb155.sub.--1.
However, the toxicity of other materials is based on toxicological
rather than nutritional studies. One way to access this information
is through their Materials Safety Data Sheet (MSDS). The silver,
gold, and copper, or bronze, sprinkles used on baked goods are
called dragees. They have small amounts of the relevant metals as
coatings but are considered non toxic by the FDA.
Advantageously, the non-toxic authentication flakes are very thin,
hence the amount of "foreign", even though non-toxic, material
introduced per pill would be very small, by way of example in
milligram or even microgram quantities. Spot-printing of the flakes
onto pills or capsules further reduces the amount of "foreign"
material.
A quick calculation based on 20 micron square by 0.5 micron thick
flakes of pure materials gives a total weight for 10,000 flakes of
these materials of about 3-10 micrograms depending on exact
composition and size of the flakes, so that less than 1%, even less
than 0.1% in most cases, of the pill consists of the authentication
flakes. This number of flakes per pill ensures that the flakes are
easy to identify on the surface of the pill.
In one embodiment, the non-toxic flakes are dispersed in a
non-toxic carrier, making a non-toxic composition for covering
pills or forming capsules cases for a medicine. Alternatively,
non-toxic composition is spot-printed onto pills or capsules thus
reducing the amount of flake material. The non limiting examples of
non-toxic carriers are gelatin, propylene glycol alginate (PGA),
agar, carrageenan, alginic acid or salt thereof, gums, such as gum
arabic, gellan gum, xanthan gum, and the like, and celluloses such
as HPMC, HPC, HEC, CMEC, HPMCP, and the like, polyvinyl
pyrrolidone, maltodextrin, polydextrose, modified starches. Other
conventionally employed polymers and resins of this type may be
employed.
As the authentication flakes are non-toxic and preferably inert,
the amount of flakes in the coating is determined by either FDA
regulation which governs the quantity of non-active material
fillers or the desire for the flakes to be non-obvious or covert.
The concentration by weight is dependent on whether the taggants
are spot printed, and whether only the tablet coating or the entire
dose weight is considered. Typically, the weight of authentication
flakes is less than 10% of the coating weight, preferably, less
than 1%, and, more preferably, less than 0.1%.
Alternatively, non-toxic flakes can be pressed into the surface of
non-coated pills or tablets.
In one embodiment of the present invention, the authentication
flakes are dispersed within the core of a pill or tablet or
capsule, essentially consisting of a biologically active or inert
material, or a mixture thereof. In this context, "essentially"
means that authentication flakes can be added to the material of
the core, amounting to no more than 5% of the weight. Preferably,
no more than 1% of the article consists of the authentication
flakes. However, it might be more if non-toxic flakes are used for
labeling very small particles, by way of example, an individual
particle in a "timed release" formulation. When the taggants are
used forensically, as part of the body of the pill, they are
dispersed through the volume of the pill or tablet or capsule. More
flakes are needed so that they can be readily located. To detect
those particles, the pill is typically dissolved and the residue
examined for the taggants.
In one embodiment of the present invention, the authentication
flakes are non-toxic inorganic taggant flakes, preferably
single-layered. Taggant flakes, also referred to as taggent flakes,
are encoded with information, either in the form of a grating
and/or one or more symbols on the surface of the flake, or in the
form of a selected shape. Multiple distinguishing effects are
possible on a flake, for example, it can be a shaped flake with a
one or two dimensional grating and a superimposed symbol. The
features work in combination to form a unique taggant. The material
too is a feature which can be subjected to analysis albeit
forensic.
In particular, taggant flakes having grating thereon are disclosed
in U.S. Pat. No. 6,815,065 in the names of Argoitia et al.; the
taggant flakes having symbols thereon, and frames or borders
embossed, etched or lasered into the flake for protecting the
symbols during the process of separating flakes from their
temporary support backing are disclosed in U.S. Patent Application
No. 20060035080 by Argoitia; both documents are incorporated herein
by reference.
In one embodiment of the present invention, the authentication
flakes are single layered metal taggant flakes, made of non-toxic
material, gold by way of example. Taggant flakes are described in
more detail hereinbelow.
Alternatively, the authentication flakes are non-toxic optically
variable flakes, in particular including a Fabry-Perot interference
structure consisting of a reflector layer, a dielectric layer, and
an absorber layer. Conventional OV flakes made with Al, MgF.sub.2
and Cr, are not recommended for ingestion, since Al and MgF.sub.2
are not desirable, and only Chromium may only be considered safe in
extremely small amounts. Care should be taken to use only non-toxic
materials. By way of example, an iron, zinc, magnesium, titanium,
gold, silver or iron reflector and an inert or food safe
dielectric, such as aluminum oxide, titanium oxide, or a silicon
oxide, can be used in non-toxic OV flakes. For the absorber layer,
chromium can be used in appropriately small amounts, or another,
better tolerated or physiologically acceptable aforementioned
metal.
Alternatively, multilayered OV flakes are all-dielectric, for
example, having alternating layers of high- and low-index materials
such as disclosed in the U.S. Pat. No. 6,815,065 to Argoitia, et
al. For example, non-toxic OV flakes are made of SiO2/TiO2
multilayers.
The authentication OV flakes can have a particular or random shape,
in the latter case the color shifting effect is used for
authentication purposes. The OV flakes having a particular shape or
symbol or grating, are referred to as OV taggants.
Advantageously, individual pills can be marked with taggants using
conventional printing or coating methods, so that special
application equipment is not required. Further, the pharmaceutical
manufacturers may carry a stock of variously encoded taggants and
apply them singularly or in various changeable combinations at
their own discretion, maintaining the coding information within
their own organization and varying it according to their needs. By
varying the location of taggants on the pill, and the combination
of taggants code used, each lot may be customized with unique
information.
Taggants having a particular shape or with surface relief indicia
or both can be produced by sputtering or evaporation onto a
pre-embossed surface, either a film carrier as currently used or a
wax layer as described in the U.S. Pat. No. 6,376,018 in the name
of a co-inventor of the present invention. It is likely that
dedicated machinery would be required for production to maintain
material purity. In the case of deposition on a wax layer, a food
grade paraffin may be used which could be incorporated directly
into the tablet coating process.
Particular types of authentication flakes are described
hereinbelow.
II. Exemplary Covert Flake
FIG. 1 is a plan view of a portion of a document 10 with a security
feature 12 according to an embodiment of the present invention. At
least a portion 14 of the security feature 12 is printed with ink
or paint including clear or colored flakes having indicia
(hereinafter "covert flakes") mixed with bulk pigment, such as bulk
pigment flakes. In one embodiment, the covert flakes have a
particular shape, such as being square, rectangular, trapezoidal,
"diamond" shaped, or round, for example. In another embodiment, the
covert flakes include a symbol and/or grating pattern, with or
without having a selected shape. Covert flakes are also sometimes
referred to as "taggent" flakes, although not all taggent flakes
are necessarily covert flakes.
Generally, the bulk pigment particles have an irregular shape. In
one embodiment, the covert flakes are distinguishable from bulk
pigment particles, including bulk pigment flakes, by their shape.
Alternatively, bulk pigment flakes have a first selected shape, and
the covert flakes have a second selected shape. Production of
shaped pigment flakes is accomplished by a variety of techniques,
such as using a patterned substrate to deposit the flake material
on the substrate and then separating the flake from the substrate
to obtain the pattern, or using a laser or other means to cut the
patterned flakes from a sheet of flake material. The selected shape
of the covert flakes may be associated with a manufacturing
facility, date of manufacture, or other aspect of the document 10,
or ink used in producing the document, for example.
A roll coater is one type of apparatus that can be used to produce
covert flakes according to embodiments of the invention. A roll of
a sheet of polymer substrate material (also known as a "web") is
passed through a deposition zone(s) and coated with one or more
thin film layers. Multiple passes of the roll of polymer substrate
back and forth through the deposition zone(s) may be made. The thin
film layer(s) is then separated from the polymer substrate and
processed into flake. Other apparatus and techniques may be
used.
Alternatively or in addition to having a selected shape, the covert
flakes may include one or more symbols. The symbol could be a
letter, number, or other marking. A symbol could indicate the
manufacturer of the covert flake, the user of the covert flake, or
a date code, for example. The symbol(s) could be embossed on a
substrate used in a roll coater prior to depositing thin film
layers that are processed into flakes, or formed on the thin film
layers after deposition, such as by laser ablation, embossing, or
etching, for example.
A pigment flake with a selected shape or symbol provides a security
feature even if it is easily observable; however, if a pigment
flake with a selected shape or symbol is not easily observable, a
counterfeiter might not even be aware that a covert flake is
present. One embodiment of the present invention uses covert
pigment flake that has the same optical characteristics as the base
pigment. The percentage of covert pigment flakes is sufficiently
small so that the covert pigment flakes are not easily found, even
under microscopic examination. For example, if an ink composition
has covert pigment flakes making up less than 1% of the total
weight of pigment (i.e. base pigment plus covert pigment), the
covert pigment flakes are difficult to find.
Another approach is to use a clear, inorganic covert flake with a
selected shape or symbol. In one embodiment, clear inorganic covert
flakes are mixed with base pigment flakes in a carrier, such as an
ink vehicle or a paint vehicle, to form a composition, such as ink
or paint. In another embodiment, the clear inorganic covert flakes
are mixed in a clear carrier to form a varnish. The index of
refraction of the carrier is sufficiently similar to the index of
refraction of the clear covert flake so that the covert flake
"disappears" in the carrier. Examples of carriers include polyvinyl
alcohol, polyvinyl acetate polyvinylpyrrolidone,
poly(ethoxyethylene), poly(methoxyethylene), poly(acrylic) acid,
poly(acrylamide), poly(oxyethylene), poly(maleic anhydride),
hydroxyethyl cellulose, cellulose acetate, poly(sacchrides) such as
gum arabic and pectin, poly(acetals), such as polyvinylbutyral,
poly(vinyl halides), such as polyvinyl chloride and polyvinylene
chloride, poly(dienes) such as polybutadiene, poly(alkenes) such as
polyethylene, poly(acrylates) such as polymethyl acrylate,
poly(methacrylates) such as poly methylmethacrylate,
poly(carbonates) such as poly(oxycarbonyl oxyhexamethylene,
poly(esters) such as polyethylene terephthalate, poly(urethanes),
poly(siloxanes), poly(suphides), poly(sulphones),
poly(vinylnitriles), poly(acrylonitriles), poly(styrene),
poly(phenylenes) such as poly(2,5 dihydroxy-1,4-phenyleneethylene),
poly(amides), natural rubbers, formaldahyde resins and other
polymers.
The clear covert flake does not typically become totally invisible
in the carrier, but becomes less visible than it is in air. If an
observer knows where to look, the clear flake typically has a
shadowy appearance, as do symbols formed in or on the clear flake.
However, if one does not know where or how to look for the clear
flake, it usually goes undetected.
In a particular embodiment, the clear covert flake has a
reflectivity in the visible range of about 30% in air, and less
than 30% reflectivity in the carrier. Thus, the clear covert flake
typically has a transmittance of more than 70% when dispersed in
the carrier, which maintains the visible characteristics of the
base pigment that the clear covert flake is mixed with or that
underlies a varnish containing the clear covert flake.
Clear, inorganic covert flakes are difficult to detect, even when
they make up more than 1% of the total pigment weight in a
composition or varnish. In one embodiment, the clear covert flake
is a single layer of ZnS heat-treated to fluoresce under UV light.
The location of the ZnS covert flake is illuminated with UV light
to identify its location, and then it is observed using visible
light, typically under a microscope at about 20.times.-200.times.,
to observe the indicia of the covert flake.
FIG. 2A is a simplified plan view of a portion 14A of a security
feature according to an embodiment of the present invention. The
portion 14A of the security feature is viewed under magnification,
typically about 20.times.-200.times., in order to see the shape of
the flakes, which are typically about 5-100 microns across, more
typically about 20-40 microns across. The security feature has been
printed with ink including base pigment particles 16 and a covert
pigment flake 18 having a selected shape, in this case a "diamond"
shape. The base pigment particles are illustrated as being
irregularly shaped flakes. Alternatively, the base pigment
particles are flakes having a selected shape. The covert pigment
flake has similar optical characteristics as the base pigment
particles, otherwise does not disturb the visual appearance of a
composition made with the base pigment particles.
When the covert pigment flake is illuminated with non-visible
radiation, such as UV or IR light or an electron beam, the covert
pigment flake glows. In a particular embodiment, the covert pigment
flake fluoresces under UV light. Illuminating the covert pigment
flake with non-visible radiation allows an observer to identify
where the covert pigment flake is located in the security feature,
even if present in very small quantities. The observer then
inspects the covert pigment flake under visible light to see the
selected shape of the covert pigment flake, or to see the symbol(s)
on the covert flake.
FIG. 2B is a simplified plan view of a portion of a security
feature 14B according to another embodiment of the present
invention. The security feature has been printed with ink including
base pigment particles 16 and a covert pigment flake 18B having an
irregular shape and containing a symbol 20, in this case a stylized
"F". Several different symbols and combination of symbols could be
used. The portion 14B of the security feature is viewed under
magnification, typically about 100.times.-200.times., in order to
see the symbol(s), which are typically about 0.5-20 microns high,
on the covert pigment flake 18B.
The covert pigment flake 18B was made by depositing one or more
thin film layers on a substrate, such as a plastic film, separating
the thin film layer(s) from the substrate, and processing the
separated thin film layer(s), such as by milling and sieving, into
the desired flakes. The covert pigment flakes are typically about
5-100 microns across, and more typically about 20-100 microns
across. The symbol 20 is typically about 0.5-20 microns tall. In a
particular embodiment, the symbol 20 is about 700 nanometers tall
and in another embodiment the symbol is about 15 microns tall. It
is generally desirable to have the symbols sufficiently close so
that most flakes have at least an identifiable portion of a symbol.
In one embodiment, symbols that were 8 microns tall were spaced
about 2 microns apart, which resulted in covert flakes having about
6 symbols per flake, on average. Symbols having bilateral symmetry
appear the same whether viewed from the top or the bottom of a
clear flake, but such symmetry is not required. In another
embodiment, symbols that were about 15 microns tall were spaced
about 4 microns apart.
The symbols are typically embossed on the substrate, and the thin
film layer(s) deposited over the embossed substrate. The surface of
the substrate, namely the symbol, is replicated in at least the
first thin film layer that is deposited on the substrate, in either
positive or negative relief. Thus, when the thin film layer(s) is
separated from the embossed substrate and processed into flake, at
least some of the flakes contain the symbol. The spacing of
embossed symbols on the flake can be selected so that essentially
every flake above a certain size will contain at least one
symbol.
The base pigment particles are illustrated as being irregularly
shaped flakes. Alternatively, the base pigment particles have a
selected shape. Similarly, the covert pigment flake 18B could have
a selected shape, in addition to the symbol 20, and a superimposed
grating, such as a diffraction grating, could be included either
over the entire flake or over selected portions of the flake, such
as over the field of the flake, but not over the symbol.
Alternatively, one type of grating is formed in the field of the
flake, and another type of grating (e.g. with different pitch) is
formed in the symbol area. The addition of a grating further
increases the difficulty of counterfeiting. The covert pigment
flake has generally the same optical characteristics as the base
pigment particles, or is present in sufficiently small quantities
so as not to disturb the visual appearance of a composition made
with the base pigment particles.
In a particular embodiment, the base pigment particles are flakes
of mica coated with a layer of TiO.sub.2 or other dielectric
material. The coating material typically has a relatively high
index of refraction. Mica is a naturally occurring mineral that is
relatively inexpensive and easily processed into flake substrate.
When mica flake substrate is coated with a layer of high-index
material of a selected thickness, a nacreous pigment flake is
obtained. Mica flake substrate can be coated with several
alternative materials using a variety of processes. Such pigments
are commonly known as "mica-based" pigments. A photocopy of an
image printed with such nacreous pigment flakes does not look like
the original, thus mica-based pigment flakes are desirable for use
to provide overt security features. However, shaping mica flake
substrate or providing a symbol on mica flake substrate is
impractical. Covert pigment flake according to an embodiment of the
present invention is mixed with the mica-based pigment to enable a
covert security feature to be included in images printed with
mica-based pigment flakes. Covert pigment flakes made of a single
layer of inorganic dielectric material, such as TiO.sub.2 or ZnS,
can have an appearance similar to a mica-based pigment if the
covert pigment flake has a thickness about five times the
quarter-wave optical thickness ("QWOT") at a selected wavelength in
the visible spectrum. Typically, a single-layer covert pigment
flake of ZnS or TiO.sub.2 intended to match the appearance of a
mica-based pigment has a thickness of about 60 nm to about 600 nm.
In one embodiment of the present invention, non-toxic single
layered taggant flakes made of inert TiO.sub.2 having a
predetermined shape and/or a symbol on the surface are used for
authentication of pills, capsules with medicine, tablets, etc. For
identification purposes, color centers are introduced into TiO2, or
it can be sensitized with dyes to enhance electro-optical activity,
most notably for photovoltaic applications. Such flakes can be
identified by fluorescence or spectrometry.
FIG. 2C is a simplified plan view of a portion of a security
feature 14C according to yet another embodiment of the present
invention. The security feature has been printed with ink including
base pigment particles 16 and a clear covert flake 22 having an
irregular shape and containing a symbol 20', in this case a
stylized "F". Several different symbols and combination of symbols
are alternatively used. Alternatively, a clear covert flake has a
selected shape, with or without a symbol.
The clear covert flake is formed from a deposited (i.e. synthetic),
inorganic thin film layer and in a particular embodiment is a
single layer of ZnS about 700 nm thick. In a further embodiment,
the ZnS flake it treated to enhance fluorescence. Alternatively,
other materials that fluoresce visible light when exposed to UV
light are used in other embodiments, such as zinc silicate,
calcium-tungsten oxide, yttrium phosphate vanadium, doped yttrium
oxide (such as with europium), and alkaline earth aluminates doped
with rare earth aluminates, to name a few. Alternatively, other
materials that fluoresce in the long UV range (300-400 nm) when
excited with low UV radiation (about 250 nm) are used. Fluorescence
is not required for all embodiments of the present invention.
In one embodiment, the material of the clear covert flake is chosen
according to the intended carrier that it will be mixed with to
obtain a selected match or mismatch of the index of refraction of
the flake in the carrier. For example, when a clear flake made from
a low-index material is mixed in a low-index carrier, the clear
flake is very difficult to see. If the low-index clear flake is
mixed in a high-index carrier, the clear flake is easier to see,
but still not generally detected by casual observation.
Single layer flakes made of inorganic materials more than about ten
QWOTs thick tend to be clear, rather than tinted or nacreous.
However, even clear flakes can impart a yellowish tinge to a
composition, such as a varnish. It was discovered that
heat-treating some clear inorganic flakes improved their
"whiteness", resulting in a superior varnish for use in covert
security applications. In a particular embodiment, clear pigment
flakes made from a single layer of ZnS about 700 nm thick were
heated in air to a temperature of 550.degree. C. for about 600
minutes to enhance fluorescence under UV light. This heat treatment
also improved the whiteness of the ZnS flake.
It is thought that trace elements remaining from the roll-coating
process contributed to the enhanced fluorescence. In particular,
NaCl was used as a release layer on the polymer substrate used in
the roll coating process. A single layer of ZnS was deposited over
the NaCl release layer, which was subsequently dissolved in water
to facilitate removal of the ZnS from the polymer substrate. It is
thought that sodium from the release layer doped the ZnS or
activated other dopants, resulting in enhanced fluorescence.
FIG. 3 is a cross section of a varnish 24 with clear covert flakes
22 dispersed in a carrier 26 according to an embodiment of the
present invention. An optional color coat 28 has been applied to an
object 30 underneath the varnish 24. The varnish 24 provides a
covert security feature to the object without disturbing its
appearance. In a particular embodiment, the optional color coat 28
is an image printed with nacreous or color-shifting pigment to
provide an overt security feature to the object. The object is a
document, product, packaging, or seal, for example. The varnish 24
enables providing a covert security feature to an object that
already has a covert security feature without significantly
altering the appearance of the object. For example, if stock
certificates have been printed with overt security features and it
subsequently becomes desirable to provide a covert security feature
to the stock certificates, the overt security feature is
over-printed with the varnish or a similar clear ink composition.
In another embodiment, an additional covert security feature is
provided to an object already having one or more covert security
features. In a particular embodiment, the clear covert flakes make
up not more than 2% of the varnish. Additional discussion regarding
varnishes is provided below in the section on experimental results.
Alternatively, the varnish 24 is a non-toxic carrier for coating
pills or tablets 30, and clear covert flakes 22 are made of
TiO.sub.2.
FIG. 4 is a cross section of a composition 25 (e.g. ink or paint)
including base pigment flakes 16 and clear covert flakes 22
dispersed in a binder according to another embodiment of the
present invention. The clear covert flakes 22 have a symbol (see
FIG. 2C, ref. num. 20'). Alternatively, the composition 25 includes
selectively shaped clear flake, with or without a symbol(s), and/or
covert pigment flake that is shaped and/or includes a symbol (see
FIG. 2A, ref. num. 18 and FIG. 2B, ref. nums. 18B, 20). In one
embodiment, the amount of clear covert flake 22 in the composition
is less than 1% of the total weight of the base pigment flake 16
and clear covert flake 22 ("total pigment weight"), which
sufficiently disperses the clear covert flakes in the base pigment
flake to make casual detection of the covert flake difficult. In an
alternative embodiment, the amount of clear covert flake in the
composition is greater than 1%.
Adding covert flake to an existing ink or paint composition
provides a covert security feature to images made of the ink or
paint. For example, ink with color-shifting pigment is used to
provide a color-shifting image as an overt security feature on a
bank note or other object. Covert flake according to an embodiment
of the present invention is added to the ink, and the resultant
mixture is used to print images that appear substantially similar
as those printed with the ink. Thus, a casual observer of the bank
note does not notice a change in the appearance of the overt
security feature (i.e. color-shifting image) after the covert
security feature is added. The indicia of the covert flake
indicates a date-of-manufacture, a printing location, and/or the
source (manufacturer) of the ink, for example.
III. Identification of Covert Flakes
FIG. 5A is a simplified plan view of a portion of a security
feature 114 printed with clear, inorganic covert flake 122
according to an embodiment of the present invention as seen under a
microscope using UV illumination. The flakes are shown in a single
layer for simplicity of illustration (compare FIG. 4). The clear
covert flake 122 fluoresces (appears bright) and is easily
distinguished from the base pigment flake 116, which appear dark
and are shown in dashed lines for purposes of illustration.
Typically, a much larger field of view is observed (i.e. lower
magnification, typically 20.times.-50.times.). A reduced field of
view is being shown for simplicity of illustration. Once the
location of the fluorescent covert flake is identified, the viewer
can "zoom-in" on the covert flake.
FIG. 5B is a simplified plan view of the portion of the security
feature 114 of FIG. 5A as seen under a microscope using visible
light for illumination. It was discovered that symbols on the clear
covert flake were not easy to read under UV light because the
fluorescence was a bulk phenomenon and obscured the symbol. When
the UV light was switched off and the clear covert flake 122 was
observed under a microscope using visible light, the faint outline
of a symbol 120 (as well as the flake) was observable. Fluorescent
covert flakes are particularly desirable when the concentration of
flakes is low. The clear covert flake 122 and the symbol 120 are
shown as dashed lines in this view to represent that they appear as
faint outlines under visible light. The base pigment flakes 116 are
shown as solid lines because they are typically prominent under
visible light. In a particular embodiment, the clear covert flake
was ZnS having an index of refraction of about 2.2 in a high-gloss
varnish that was first observed under UV light, and then the symbol
on the flake was read using visible light at a magnification of
100.times.
A similar result is expected for covert pigment flakes that
fluoresce under UV light or other non-visible radiation. For
example, covert pigment flake dispersed in base pigment flake
having similar visual characteristics is difficult to detect when
the covert pigment flake is sufficiently dilute. In one embodiment,
the covert pigment flake has a selected shape that is observable
under UV light. In another embodiment, the covert pigment flake has
a symbol that is not easily observable under UV light, but is
observable under visible light. The location of the covert pigment
flake with the symbol is identified using UV light and then the UV
light is switched off and the symbol is read using visible
light.
Alternatively, a material that fluoresces at a shorter wavelength
when illuminated with light at a longer wavelength is used to
fabricate covert flakes or covert pigment flakes. It is believed
that this type of fluorescence would be less easily noticed by a
counterfeiter, enhancing it use in covert security applications. In
one embodiment, near infrared or infrared light is used to
illuminate covert flake or covert pigment flake to fluoresce in the
visible range.
IV. Experimental Results
Prior to developing clear covert flake or single-layer covert
pigment, various alternatives were evaluated. A test standard using
100% magenta-to-green optically variable intaglio ("OVI") pigment
flake was produced and measured. All taggent samples had a grating
pattern of 2000 lines/mm, which makes the taggent flakes easier to
distinguish from the base flake (i.e. locate) and more difficult to
counterfeit. The grating pattern did not induce diffractive
properties to images printed with the test compositions. It is
believed that the low portion of the taggent flakes in combination
with not being well oriented to the viewer avoided a diffractive
property from occurring. In a particular embodiment of the present
invention, a grating pattern was included on taggent flakes with
symbols. The symbols were identifiable under a microscope at a
first magnification, but the grating pattern was not easily seen at
this first magnification. The grating pattern was seen at a higher
magnification. It is believed that including such a grating pattern
further enhances the covert nature of the taggent flake because a
counterfeiter might see the symbol under microscopic examination,
but not see the grating pattern, and hence not include it in a
counterfeit article.
The first test sample ("sample 1") contained 90% (by weight) of the
conventional magenta-to-green pigment flake mixed with 10%
magenta-to-green OVI pigment flake including symbols ("taggent
flake"). The taggent flakes were easy to detect by routine
microscopic inspection, and the color performance of the mixture
was the same as the test standard because the color of the taggent
flake was well matched to the color of the base flake. However,
close color matching involves careful monitoring of the production
of the taggent flake. Similarly, a new optical design for each
color of taggent flake would generally be used to match each color
of base flake. Thus, this approach does not provide a generic
taggent flake that can be mixed with a variety of colored base
pigments.
A simpler approach is to use a standard taggent flake design that
can be used with many different colors of base flake. Single-layer
MgF.sub.2 taggent flake (was mixed with the magenta-to-green OVI
base pigment, the taggent flake making up 10% of the total pigment
weight ("sample 2"). As with the color-matched OVI, color
performance was essentially identical to samples produced with 100%
base OVI pigment flake. However, the MgF.sub.2 flakes were
difficult to detect under routine microscopic examination, even at
a concentration of 10%.
"Silver" (aluminum) taggent flake was also evaluated. Fabrication
of silver flake is relatively simple and these flakes were very
easy to detect at a concentration of 5%. It was hoped that silver
taggent flakes would be able to be mixed with many colors of base
pigment. However, the color performance of an intaglio blend
containing only 5% silver taggent flake mixed with the
magenta-to-green OVI base pigment ("sample 3") was poor. Thus,
silver taggent flake may be useful in certain compositions, but
appear to degrade the color performance of at least some base
pigments.
Finally, clear taggent flake was made from a single layer of ZnS.
Production of this flake is relatively easy, and detectability at
10% concentration was easy, which is to say it was more difficult
than detecting the OVI taggent flakes, but much, much easier than
detecting the MgF.sub.2 taggent flakes. An intaglio blend with 10%
ZnS flake and 90% magenta-to-green OVI flake ("sample 4") was
compared against the test standard. The color performance was
nearly equal, with a slight (about 3%) decrease in chroma. The
persons involved in this subjective comparison are quite
experienced in evaluating color performance of optically variable
pigments, and used a side-by-side comparison against a standard. It
is believed that 10% of this flake added to an existing ink or
paint composition would preserve the color performance sufficiently
so that an average observer would not notice any change. The ZnS
clear taggent flake appears able to be added to a large number of
colored pigments, including optically variable pigments without
noticeably altering the appearance of compositions made with the
colored pigments, and hence enables a generic taggent flake.
The measured optical performance of the samples described above is
provided in Table 1:
TABLE-US-00001 TABLE 1 Optical Performance of Intaglio Blends
Sample # L* a* b* C* h Test standard 49.27 40.32 -31.05 50.89 322.4
Sample 1 49.08 40.25 -30.87 50.73 322.51 Sample 2 49.42 40.62
-31.04 51.12 322.61 Sample 3 52.67 35.26 -27.26 44.57 322.29 Sample
4 49.66 39.22 -29.85 49.29 322.72
Clear ZnS flake for use as a taggent or covert taggent was also
evaluated in varnish compositions. It was determined that in some
instances almost one-third of the varnish composition could be
clear flake with almost no change in the perceived appearance of
the varnish composition. A high-gloss varnish base was used to make
the varnish compositions and the varnish compositions were applied
to white card stock of the type normally used for color evaluation
of inks and paints. All varnish compositions were compared against
a test standard of the varnish base without clear flake.
In the first varnish composition, 3% of as-deposited (i.e. not
heat-treated for clarity) single-layer ZnS looked essentially
identical to the test standard. A second varnish composition having
5% single-layer as-deposited ZnS flake was barely noticeably
different when compared against the test standard, but it is
believed that a casual observer would not notice the slight amount
of yellowing. A third varnish sample with 10% single-layer
as-deposited ZnS flake exhibited a noticeable change in appearance
when compared against the test standard, and it is believed that
some casual observers would notice a field printed with this
composition on a very light background. However, this composition
might be useful for printing on non-white substrates, such as bank
notes or off-white stock certificates, where the slight yellowing
would be less likely to be noticed. Alternatively, a non-gloss
varnish base is used to further reduce likelihood of detection when
used as a covert security feature. A fourth varnish sample with 15%
single-layer as-deposited ZnS exhibited noticeable yellowing, even
without a side-by-side comparison with the test standard.
Single-layer ZnS flake was heat treated to clarify ("bleach") the
flake. The flake was heated to 200.degree. C. for two hours in air.
Heat treating ZnS flake to enhance fluorescence (550.degree. C. for
10 hours in air) also bleaches the flake, but bleaching can be
achieved with the shorter heat treat. A varnish composition using
20% single-layer bleached ZnS showed almost no perceptible color
change. Thus, it is believed that at least 10% of unbleached
single-layer ZnS flake and at least 20% of bleached single-layer
ZnS flake could be added to a high-gloss varnish base as a covert
taggent.
ZnS is further desirable as a taggent flake because, unlike some
flake including a metal (e.g. aluminum) layer, ZnS is durable in
the presence of water, acid, base, and bleach. Unlike some organic
flake, ZnS is also durable in the presence of organic solvents and
sunlight.
FIG. 6 shows the color travel for a test sample prepared with an
ink, and for test samples prepared with the ink in combination with
covert pigment flakes according to an embodiment of the present
invention. The color plots are according to the CIE La*b*
conventions. The illumination and viewing angles were ten degrees
off from the specular angle to avoid the strong gloss component
associated with clear-coated samples. The samples were
characterized using eleven angles of illumination/viewing from
15.degree./5.degree. to 65.degree./55.degree. in 5.degree.
increments. The first point of the curve (i.e. the upper left
point) corresponds to the 15.degree./5.degree. datum, and the last
(i.e. eleventh) point corresponds to the 65.degree./55.degree.
datum.
A first curve 600 shows the measured color travel for a test sample
prepared with blue-to-green optically variable pigment flake. A
second curve 602 shows the measured color travel for a sample
prepared with 95 weight percent blue-to-green optically variable
pigment flake and 5 weight percent of single-layer ZnS flake about
700 nm thick and having an average particle size of about 20
microns. Symbols on the flake were about 8.times.6 microns,
separated by about 2 microns of field. The weight percent is the
percent of the total weight of the flake used to prepare the ink
composition for the sample. A third curve 604 shows the measured
color travel for a sample prepared with 90 weight percent
blue-green optically variable pigment flake and 10 weight percent
of the same ZnS flake used in the sample associated with the second
curve. These curves illustrate that very similar optical
performance is achievable for ink compositions having up to 10
weight percent covert flake. In particular, the color travel is
nearly identical for all three samples, and the chroma is only
slightly less for the sample made with 10% clear covert flake.
Thus, a covert flake according to an embodiment of the present
invention is added to an existing optically variable ink to form a
composition to provide a covert security feature without
significantly altering the appearance of images printed with the
composition.
V. Exemplary Methods
FIG. 7 is a simplified flow chart of a method 700 of providing an
object with covert flakes according to an embodiment of the present
invention. Covert flakes that fluoresce under non-visible radiation
are mixed in a carrier (step 702) to provide a composition, such as
ink or paint, in which the covert flakes are not easily detectable
by observation under visible light. In one embodiment, the covert
flakes are clear covert flakes that have a symbol and/or a selected
shape. In a further embodiment, the composition includes base
pigment flakes or particles. In another embodiment, the covert
flakes are covert pigment flakes that have a symbol and/or a
selected shape. The composition is applied to the object (step 704)
to provide a covert security feature. In one embodiment, the
composition is applied using a printing step, such as a gravure,
flexographic, offset, letterpress, intaglio, or screen printing
step. In another embodiment, the composition is applied using a
painting step, such as a rolling, dipping, brushing, or spray
painting step.
After providing the covert security feature, the covert security
feature is observed by illuminating the object with non-visible
radiation (step 706) to cause the covert flakes to fluoresce and a
covert flake is identified (step 708). If the composition has base
pigment flakes or particles that also fluoresce, it is understood
that the covert flakes fluoresce significantly more or less, or at
a different color, than the base pigment flakes or particles so
that the covert flakes stand out in the composition and are easily
identified. The identified covert flake is observed (step 710) for
a security marking. In one embodiment, the covert flake has a
selected shape and is observed while the object is illuminated with
non-visible radiation. In another embodiment, the covert flake
includes a symbol, and the covert flake is observed using visible
light after the step of identifying the covert flake using
non-visible radiation. In a particular embodiment, the step of
observing one or more symbols on the covert flake is done under
magnification of 50.times.-200.times. While the invention has been
described above in terms of various specific embodiments, the
invention may be embodied in other specific forms without departing
from the spirit of the invention. Thus, the embodiments described
above illustrate the invention, but are not restrictive of the
invention, which is indicated by the following claims. All
modifications and equivalents that come within the meaning and
range of the claims are included within their scope.
* * * * *
References